Blue vat dye and process of making same.



s'rnrrns A NT orrion;

or rnAnxron'r-oN-rEn-Mnn; GERMANY, 'Assmnon ro cAssELLA ooLon conrnnr;or NEW YORK, n. Y. 1

wen? {stun VAT on s rnocsss OF MAKI SAME- 9563482 Specification ofLetters Patent.-

.HoDrawhg. April-i catihn flldQ-June 25, 1909.'-Seria1 No. 504,340.(Specimens) result it is necessary to 55 Patent No. 919,572.- Inorder toobtain this scribed in Edited-,Stdtsfiatjgt No. 919572,

" Patented spri es; 19 10.

use in the production- -T all whom it may concern:

Be it known that I, RICHARD Henz, doctor of the dyest-ufis an alkalinepol sulfid eom of philosophy, :1 subject of the Kingdom of tainin a highpercentage of sulfur, and it' v Prussia, and a resident ofFrankfort-on-theis pro era' ble to carry out the process in the 5 Main,in the Province of Hesse-Nassau and presenee ioi a suitable solvent suchas ethyl- Kingdom of Prussia, Germany, have inventmethyl-211061101- Itis 31-30' p fer to ed some new and useful Improvements in the use theproducts of condensation" or their *P'roduotion of Blue Vat Dyestuffsand Procleuco compounds ina ure state: esses of Making Same, of whichthe follow- I have 'found the fol'owing'method suit, 0 ing is a fulldescription. 7 able and efl'ectivez- 1 In the United States Iatent No.919572 of Ex mpl 1 0 kilos sodium sulfid crystals Louis Haas there aredescribed blue sulfid and 64: kilos Su fu are-heated for a Shortdyestuffs resulting from thereaction of: t t until the \Vllolfisulfufvpoly'sulfids on the products of condensation 'd ed and the g ea erportion of the. of -p.nitr osophenol with carba-zol in the presystawater f th sodium sulfid 1s evap ence of concentrated sulfuric acid. Ihav rated. To the sodium tetrasulfid thusiormed now found that accordingto the conditions are e added 100 kilos fi ly ground .app1ied-in theirmanufacture, different prodfi pr f r b y o ers of S11 fur, and 400 notemay be obtained whi h diff 653611-, liters ofethyl alcohol. The mass. isthen ti ll f o h other 7 i res t t their heated for about 2 to 3 hourswith the reflux solu ility in dilute sodium su fid solution. condenseruntil the gh y ulfurebed i m If, for instance,'the raw melt, obtained,as Sulfid 15 formed; then i the y described in the example of theaforesaid P b are d mgr qtu y the United States patent, is heated with adilute followmg formula? t sodium sulfid solution, a great part of thecolorin matter goes into solution with a I I greenis brownv color,whereas a certain amount remains'undissolved. The dyestuff f t t ilvgvehich is distsogegl by thg sodilum sulfid can I J precipi te rom t eso ution by the well-lmown methods. It shows the properties of the'colprdescribed in the ubove-men- *tioned United; States patent. I havefurther and the 9 e sthereupon boned 9 discovered that the part of themelt, being abort hou h the flux condenser difiicultly soluble in dilutesodium sulfid so- Whlle mg- 9 2 leactloll i 510111 -';l"-lution, treatedreducing agents 'as the Zl-l COhOl IS d'lstllled OH, and the .m/mmonlyused f ducing ind go d' residue washed with water and filtered Y.othervat colors, such as; .for instance, an h p s t obtalfled 15 thenheated lk li fl ti f diu h d lfit i with a solution of sod um sulfidcrystals, dissolved with a pure ellow'color, forming w y t UQ Sulfur andthe a vat. Cdtton is dyed from such av vet i small amount 0 the easilgsoluble sultid -fu11 dee blue shades which are distin y fi ngm u yormedare d1s-"- guishedy their excellent fastness to wash- Solved. It" thenfiltered== &gfl1n, .the unmg, light, hnd chlor. If these dyeings aredlssolved 5141? PW P. i g Pu Vat aftertreated on the d ber with weaklyoxidiz y fil flrled, 1 1838, dark blue powder I ing agents" brightershades of the same -:fast- }YIbh & met l 0 luster. It is'almostinsoluble 11855 r bt i d, 1 h f rth di 1n the usua prganicsolve'nts, butdissolves d th t th d tip f d t ff f m with a dark reen color inconcentrated sulthe products 0? condensation o paranitroso- F W 9 191changesto abrigh phenol and carbazol 'canbe carried-out in greemsh 9 b-h t l g h {1616; 7 thu h manner th t th difii ltl l bl water. It is1nso uible m caustic allrahes and vat dyestuffs are almost x l ively rbut little soluble n' diliitealkahne sulfid duced, besides comparativelysmall amounts Q P y Whlohpro el'ty 1t can easily be of the easilysoluble color of United States dIStmgUIShQd' om @hfi isl lfid dyestufftion of alkaline sulfid substantially. as de-.

and forms, if treated wit-f1 "suitablgredue ng agents, preferablywith-,a

drosulfite solutions, a "yellowish colo'i'edf vat,

shades ofexcellent. festness,

from which cottongis dyed in deep blue,

Having now, particularly described and ascertained the nature of mysaidinvention,

and iirwh'at manner-the same is to be per-- formed, Ijleclar e tliat'what I claim is "1, The manufacture or production of fast blue vatdyestu-tfswhich consists in first condensing plnitrosophenol withcarbazol, heat-' ing the product thus obtained with alkaline *pqysulfidsin the usual manner and finally separating the val; holor from thesoluble dyes bv treating the raw meltwith a soluusual manner and finallyseparating the wit. color from the soluble dyes by treating the'rawpflhltwith-a solution of alkaline sulfid suli'tantially asdescribed,- 3. The-manufacture or-pf'oduction of fast bluc vatdyestufi's which consists-in first condensing p.nitro'sophenol withcarbazol and heating the product so; obtained with an alkalinepolysulfid containin a; high percent age of sulfur and prefera 1y thepresence ktilin Sbailyn of a suitable Solvent, especially alcohol,substantially as described.

- '4.'. '1 he manufacture or-producti'on'of fast blue vat'dyestufiswhich consists infirst cond'ensing .nitrosophenol with carbazo1, reducing t e' product and-'heating-the leuco compound so produced with analkalinepol sulfid containing a high percentage of sul ur andpreferablyin the presence of a suitable 'solvent,'e'sE'ecially alcohol, allsubstantially as descri ech- 5. Asa newarticle of manufacture the newblue vat dyestuffs deri ed from the products of condensationof"p.nitroso 'henol and carbaz'ol ortheir leuco compoun s, be

in difiicultly soluble in a dilute alkaline sufid solution andrepresenting in a dry state a dark blue powder with a metallic aspectalmost in'soluble'in the usual organic solvents, soluble with a darkgreen} color in concentrated sulfuricfacid, soluble witha pure yellowcolor in warm alkaline hydrosulfitesoluti'ons, forming avat, and dyeingcotton in suchvatfull deep blue shades fast to washing, light, andchlorin, substantially as. described.

f In wltness whereof I have hereunto 'slgned my name this 11th day ofJune 1909, in the presence of two subscribing witnesses.

' I i RICHARD HERZ.

Witnesses: I

JEAN GnUNn,

' .CARL Gunmen.-

